N-アルキル基のガスクロマトグラフ分析

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A new reaction equipment for rapid determination of alkoxyl groups by gas chromatography had been reported by the authors {This journal, 18, 608 (1969)}. In this paper, the same equipment was used for the determination of N-alkyl groups, and experimental conditions for the differentiating determination of alkoxyl and N-alkyl groups was also investigated. The less volatile reagent, KI-H3PO4, was recommended for the formation of tertiary ammonium salt of the sample and its pyrolysis in the closed system. Following procedures are recommended, and analytical results are shown in Table II. (1) Samples containing N-alkyl groups alone: Immerse the pre-column III in Fig. 2 into a Dewar bottle containing liquid oxygen. Weigh sample (25 mg) accurately into the reaction vessel, and add successively 400 mg of KI, 0.05 ml of H3PO4 and 2μl of methyl cyclohexane as an internal standard. Assemble the reaction vessel to the equipment as shown in Fig. 2. Heat the vessel stepwise as follows : at 250°C for 30 min., at 300°C for 10 min., and at 350°C for 5 min. After each heating step, collect the reaction products in the pre-column III by turning the four-way cock. Remove the Dewar bottle and heat the pre-column at about 120130°C. Introduce the collected reaction products into a gas chromatograph. Calculate each alkyl iodide content by using the internal standard method. (2) Samples containing both alkoxyl and N-alkyl groups: Heat the pre-column III at 120130°C. Weigh sample and add KI-H3PO4 and methyl cyclohexane as described above. Heat the reaction vessel at 140150°C for 20 min. After heating, turn the four-way cock and introduce alkyl iodide formed from alkoxyl group with carrier gas into a gas chromatograph. After one minute, turn the cock, and cool the pre-column III with liquid oxygen. Heat the reaction vessel. at 300°C for 20 min. and then at 350°C for 10 min. Procedures after heating are the same as in (1).
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N-アルキル基のガスクロマトグラフ分析

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